2-乳酰氨基苯甲酸的合成与有关物质测定

Synthesis and contents determination of the related substances of 2-lactoylaminobenzoic acid by RP-HPLC

目的合成2-乳酰氨基苯甲酸,并建立其有关物质的定量测定方法。方法 2-乳酰氨基苯甲酸以邻氨基苯甲酸甲酯为起始原料,经乳酰化后水解制成;有关物质测定采用RP-HPLC法,Diamonsil C18(250 mm×4.6 mm,5μm)色谱柱,以乙腈-体积分数1%乙酸水溶液为流动相,梯度洗脱,检测波长为250 nm。结果 2-乳酰氨基苯甲酸合成总收率为61.5%,其成品中有关物质总量低于0.5%,杂质A、B、C及单一未知杂质的含量质量分数均小于0.1%。结论 2-乳酰氨基苯甲酸合成与纯化工艺简单、成品纯度高;有关物质测定方法简单、灵敏、专属、耐用,可用于2-乳酰氨基苯甲酸有关物质的测定。

Objective To study the synthetic method of 2-lactoylaminobenzoic acid and develop an RP-HPLC method for the separation of 2-lactoylaminobenzoic acid and its related substances. Methods 2-Lactoylamino-benzoic acid was synthesized after lactylation and hydrolysis using methyl anthranilate as starting material. The analysis was conducted on Diamonsil C18 column （250 mm ×4. 6 mm,5 μm） with a mobile phase of acetonitfile-water containing 1% acetic acid by gradient elution at a flow rate of 1.0 mL· min^-1. The detection wavelength was set at 250 nm. Results 2-Lactoylaminobenzoic acid was synthesized from methyl anthra- nilate in 61.5 % overall yield, and its purity was not less than 99.5 %. The impurities A, B and C had been found with levels below 0. 1% in the raw material. Conclusions The method of synthesis and purification is simple with high purity of 2-lactoylaminobenzoic acid. The RP-HPLC method is simple, sensitive, accurate and reproducible. It can be used for the detection of related substances in 2-lactoylaminobenzoic acid.